HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 86686018, compound → HCID 86686019, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 86686018 | HCID 86686018 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Product | HCID 86686019 | HCID 86686019 | 38.4% |
Reaction Steps
A solution of 3-(6-chloro-pyrazin-2-yl)-piperidine-1,3-dicarboxylic acid 1-tert-butyl ester 3-ethyl ester (350.1 mmol) in THF (360 mL) and 1.5 N aqueous NaOH (360 mL) was heated at 80° C. for 5 hr. After it was cooled to room temperature, the aqueous layer was separated and then carefully acidified to pH=5 by the addition of 1 N aqueous HCl solution. The resulting mixture was extracted with DCM (300 mL×3) and the combined organic layers were dried over anhy. Na2SO4, filtered and concentrated under reduced pressure to give a crude tile compound (46 g), which was used directly in the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09133158B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-46698c3618f34adbbc0b05e2eae696ff |
| Source note | uspto-grants-2015_09 |